简便的^(13)C标记甘氨胆酸的合成方法  

A Convenient Method for Synthesis of ^(13)C Labelled Glycocholic Acid

作　　者：徐仲杰[1] 卢伟京[1] 李孝武[1] 卢浩[1] 李帅[1] 李美华[1] 吴开成[1] 

机构地区：[1]上海化工研究院,上海200062

出　　处：《精细化工》2010年第12期1216-1219,共4页Fine Chemicals

基　　金：国家高技术研究发展计划项目(2008AA02Z427)~~

摘　　要：该文"一锅煮"合成13C标记甘氨胆酸。即以氯甲酸异丁酯为活化试剂,甘氨酸-1-13C和胆酸直接缩合制备甘氨胆酸-甘氨酰基-1-13C,合成产品使用HPLC、LC-MS和1HNMR等进行分析。优化的合成条件为:n(氯甲酸异丁酯)∶n(胆酸)∶n(甘氨酸)∶n(三乙胺)=1∶1∶1∶1,反应温度10℃,反应时间1 h,13C标记甘氨胆酸收率82.4%(以甘氨酸-1-13C计),13C丰度达99.1%atom13C,光学纯度99.2%,w(甘氨胆酸-甘氨酰基-1-13C)=97.7%。With isobutyl chloroformate as the active agent,glycocholic acid-glycyl-1-13C,a 13C-breath test substrate and applications in clinical practice,was synthesized by ＂one pot＂ method of the condensation of glycine-1-13C directly with cholic acid.13C labelled glycocholic acid was characterized by HPLC,LC-MS and 1HNMR.The yield of 13C labelled glycocholic acid was 82.4%（based on glycine-1-13C）,with 99.1% atom 13C abundance,99.2% optical purity and 97.7% chemical purity,at the optimized conditions,which were n（isobutyl chloroformate）∶n（cholic acid）∶n（glycine）∶n（triethylamine）=1∶1∶1∶1,10 ℃ reaction temperature and 1 h reaction time.

关 键 词：甘氨胆酸-甘氨酰基-11-3C 稳定同位素标记 13C-呼吸试剂 

分 类 号：TQ421.7[化学工程] O621.35[理学—有机化学]